CN106588574B - A kind of slurry bed methyl alcohol synthesizing process - Google Patents
A kind of slurry bed methyl alcohol synthesizing process Download PDFInfo
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- CN106588574B CN106588574B CN201611062891.9A CN201611062891A CN106588574B CN 106588574 B CN106588574 B CN 106588574B CN 201611062891 A CN201611062891 A CN 201611062891A CN 106588574 B CN106588574 B CN 106588574B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/15—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively
- C07C29/151—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively with hydrogen or hydrogen-containing gases
- C07C29/152—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively with hydrogen or hydrogen-containing gases characterised by the reactor used
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Abstract
The present invention relates to a kind of slurry bed methyl alcohol synthesizing process, it is characterized by comprising following step: the unstripped gas from upstream forms gaseous mixture after mixing with circulating air, the shell side for entering reactor after heat exchange from bottom, contacts with the catalyst slurry in shell side and is reacted；Bubble point boiler water enters the tube side of reactor；It reacts the reaction gas generated to be discharged from the top of reactor, be separated into separator；Isolate it is non-gaseous the reactor is returned out of reactor top gas-phase space, enter in gas-liquid separator after the gas phase isolated i.e. crude carbinol synthesis gas heat exchange, as the circulating air after the pressurization of the gas phase isolated, the liquid phase isolated is crude carbinol；When catalyst abrasion reaches setting value, catalyst slurry is extracted outward from reactor；Fresh catalyst slurry is filled into the reactor shell side.The present invention does not need parking can more catalyst changeout in time.
Description
Technical field
The present invention relates to methanol synthesizing process, refer specifically to a kind of slurry bed methyl alcohol synthesizing process.
Background technique
Currently, home and abroad, which is substantially all using coal and natural gas as raw material production methanol, uses gas-solid phase catalytic, due to
Methanol-fueled CLC is a stronger exothermal reaction process, and gas-solid-phase catalytic reaction device is limited by conducting heat, bad adaptability, instead
It answers the content of CO in device import reaction gas to have to control in reduced levels, is usually no more than 16%, synthesis gas once passes through instead
Answer the conversion ratio of device also not high, therefore middle methanol content of working off one's feeling vent one's spleen is not also corresponding high, a large amount of unreacting gas must be recycled,
Power consumption is very big.
Methanol-fueled CLC is carried out using slurry bed technique, contains gas, liquid, solid three-phase in reactor, synthesis gas is through being suspended in liquid
Finely grained catalyst effect in phase heat carrier, reaction generates methanol under certain temperature and pressure.It is used in liquid phase synthesis
Thermal capacitance is high, the big inert fluid of thermal coefficient, can make that bed reaction temperature is easily controllable, synthetic reaction of methanol is in isothermal item
It is carried out under part, work off one's feeling vent one's spleen middle methanol concentration and conversion per pass can be improved, so that using high concentration reactive component (CO, H2) tool
There is feasibility.Conversion per pass improves, so that the treating capacity of unreacting gas greatly reduces, the circulating flow rate of return subtracts significantly
It is few, the circulation work done during compression of unconverted synthesis gas is substantially reduced, the energy consumption of methanol-fueled CLC process reduces.Circulation work done during compression is reduced, is mentioned
The high selection rate of process and the quality of product methanol.
CN102850182A discloses a kind of slurry bed system crude carbinol synthesis system, and the catalyst in paste state bed reactor is made
Under, reaction gas, which generates, generates gas, first through cyclone separator initial gross separation atent solvent and catalyst, then through heat exchanger boiler
The cooling generation gas of water supply, byproduct steam, the atent solvent Returning reactor condensed, and on the return line of atent solvent
Setting atent solvent makes up line.The technology reaction heat removes lag, and reaction temperature is higher, and conversion per pass is lower, easily carries secretly
Atent solvent is to downstream；And catalyst can not be replaced online, and more catalyst changeout fashionable dress, which is set, to stop, and influence device economy effect
Benefit.
Summary of the invention
There is provided that a kind of conversion per pass is high, reaction the technical problem to be solved by the present invention is to the status for the prior art
Easy control of temperature and can more catalyst changeout online slurry bed methyl alcohol synthesizing process.
The technical scheme of the invention to solve the technical problem is: the slurry bed methyl alcohol synthesizing process, feature
It is to include the following steps:
Unstripped gas from upstream forms gaseous mixture after mixing with circulating air, heat exchange to after 180 DEG C~220 DEG C from bottom into
The shell side for entering reactor is contacted with the catalyst slurry in shell side and is reacted；Bubble point boiler water enters the tube side of reactor；Control
Making the reaction temperature in the reactor shell side is 200 DEG C~240 DEG C, and reaction pressure is 4MPaG~10MPaG, gaseous mixture air speed
It is 1200-H~4000-H, catalyst quality score are 0.25~0.4；
It reacts the reaction gas generated to be discharged from the top of reactor, be separated into separator；That isolates is non-gaseous
The reactor is returned out of reactor top gas-phase space, enters gas after the gas phase isolated i.e. crude carbinol synthesis gas heat exchange
In liquid/gas separator, the gas phase isolated is forced into after 4.1MPaG~10.1MPaG as the circulating air, and the liquid phase isolated is
Crude carbinol；
In reaction process on periodic analysis different height position catalyst slurry solid content and size distribution, reach abrasion
When setting value, catalyst slurry is extracted outward from the middle and upper part of reactor catalyst bed；Extraction amount or maximum are calculated when reaching
Stop extracting catalyst slurry from inside to outside from the reactor when extraction amount；
The slurries of extraction are filtered, atent solvent and catalyst granules are isolated；
By fresh catalyst slurry be forced into higher than after reactor bed operating pressure 0.1MPa from bottom be sent into described in
In reactor shell side；The additional amount of the fresh catalyst slurry is suitable with the catalyst slurry liquid measure extracted.
It is preferred that the unstripped gas that the unstripped gas temperature is 20 DEG C~40 DEG C, pressure is 4MPaG~10MPaG, hydrogen-carbon ratio (H2-
CO2)/(CO+CO2)=2.05~2.15；The circulating air temperature is 45~70 DEG C, pressure is 4.1MPaG~10.1MPaG, is mixed
Close mole composition (H of gas2-CO2)/(CO+CO2)=3~5, recycle ratio 0.7~1.1.
It is preferred that controlling the conversion per pass 25%~40% of the conversion per pass 65~80% of the CO of the reactor, CO2.
In above-mentioned each scheme, the processing methods of the spent catalyst slurries of extraction can be with are as follows:
The catalyst slurry extracted out from the reactor shell side is introduced into settling tank and is settled；The liquid phase isolated is i.e. lazy
Property solvent send to catalyst preparation tank, as the atent solvent of fresh catalyst, the discharge of the catalyst granules that settles out.
Alternatively, preferably, the catalyst slurry extracted out from the reactor shell side, which is introduced into cross-flow filter, to carry out just
The separation of solid and liquid of step, the liquid phase isolated are sent in catalyst preparation tank by first pipe；Catalyst slurry after concentrate into
Enter and carry out smart filtering in filter, the liquid phase isolated enters the catalyst preparation tank, and catalyst granules forms filter cake discharge.
In above-mentioned each scheme, the preferably described bubble point boiler water comes from drum, and the steam that the reactor tube side generates returns
The drum；Preferably, it can also be equipped with pump in the connecting pipeline between the drum and the tube-side inlet of the reactor,
To enhance heat-transfer effect.The high-quality saturated vapor of by-product, energy conservation and consumption reduction effects are good simultaneously in Production of methanol.
It is characterized in that the catalyst is the slurry bed system methanol synthesis catalyst that activation temperature is 160~250 DEG C；Such as
The JTC-4 type methanol synthesis catalyst of Research Institute of Nanjing Chemical Industry Group exploitation, the methanol synthesis in slurry reactor of Institutes Of Technology Of Taiyuan is copper-based to urge
Agent, etc..
Prepared in above-mentioned each scheme catalyst slurry solvent can select molten boiling point is high, volatility is small, it is not easy to foaming, change
Learning performance stabilization, will not impregnate catalyst activity component out and being free of makes the harmful substance of catalyst poisoning, has good selection
The inertia liquid phase carrier of property, solvent is to the H in synthetic raw gas2、CO、CO2Etc. components solubility it is big, to Methanol product and
H2O solubility wants small；It is preferred that the alkane of carbon number 16~20 is main Witon mineral oil or atoleine.
Compared with prior art, slurry bed methyl alcohol synthesizing process provided by the present invention has an advantage that
1, reactor bed is conducted heat, and is easy to control bed temperature, is not in hot-spot, to catalyst and will not be set
It is standby to cause damages, can make bed isothermal operation under preferable reaction temperature, this preferable temperature taken into account chemical balance and
The motive force of reaction rate；Meanwhile high concentration reactive component (CO, H can be used2), H in reaction gas2Excessive, CO is control component,
And CO concentration can only generally control within 16% in the prior art.
2, conversion per pass is high, and circulating flow rate is small, greatly reduces construction investment and plant energy consumption；
3, spent catalyst is convenient to replace online, avoids economy damage caused by device parking more catalyst changeout
It loses.
4, reactor head is provided with widened segregation section and demister, is provided with cyclone separator after reactor, can
Removal methanol generates catalyst and inert carrier liquid phase medium in gas to the maximum extent.
Detailed description of the invention
Fig. 1 is the process flow diagram of the embodiment of the present invention 1；
Fig. 2 is the process flow diagram of the embodiment of the present invention 2.
Specific embodiment
The present invention will be described in further detail below with reference to the embodiments of the drawings.
As shown in Figure 1, reactor 2 used in the slurry bed methyl alcohol synthesizing process is heat exchanger structure, including top
Gas-phase space 21 and the reaction zone of lower part 22；It is equipped with heat exchanger tube in reaction zone 22, walks heat transferring medium i.e. bubble point boiler water in tube side,
Tube-side inlet connects the boiler water out of drum 4, the steam inlet of tube side outlet connection drum 4；Catalyst is filled in shell side
Slurry；Shell side inlet is connected at least one gas distributor.
Include the following steps:
From the fresh feed gas that upstream temperature is 20 DEG C~40 DEG C, pressure is 4MPaG~10MPaG, main group becomes
H2, CO and CO2, hydrogen-carbon ratio (H in unstripped gas2-CO2)/(CO+CO2)=2.1 with temperature are 45~70 DEG C, pressure 4.1MPaG
Gaseous mixture is obtained after the circulating air mixing of~10.1MPaG；Mole composition (the H of gaseous mixture2-CO2)/(CO+CO2)=4, recycle ratio
0.9。
Gaseous mixture enters preheater 1 and methanol generates gas and exchanges heat to 180 DEG C~220 DEG C, reaches the active temperature of catalyst
Afterwards, out of, the gas distributor of bottom enters paste state bed reactor 2 shell side, gas is bottom-up in shell side after being evenly distributed
Flowing, contacts with the catalyst slurry being seated in shell side, reacts.
Catalyst in the present embodiment uses the JTC-4 type methanol synthesis catalyst of Research Institute of Nanjing Chemical Industry Group exploitation, catalysis
The effect of agent ascending air in reactor, approach are evenly distributed in atent solvent atoleine, and catalyst granules partial size is
0.1~0.2mm, catalyst quality score 0.25~0.4.
When the scale of methanol-fueled CLC increases, paste state bed reactor is also increased accordingly, and a gas distributor is not able to satisfy and wants
When asking, settable multiple gas distributors.
Control 200 DEG C~240 DEG C of reaction temperature, reaction pressure 4MPaG~10MPaG of paste state bed reactor 2, air speed
1200-H~4000-h；Bubble point boiler feedwater enters anti-by density contrast, that is, pressure difference between saturated vapor after saturated water and vaporization
Device is answered, drum 4 is returned after taking heat, generates 0.6MPaG~1.6MpaG saturated vapor.
In order to overhaul heat-exchanging tube bundle, when methanol-fueled CLC scale is smaller, when 2 diameter of paste state bed reactor is smaller, in reactor
Setting disassembly flange in heat removing tube inlet and outlet nozzle overhead cylinder section；When the scale increase of methanol-fueled CLC, paste state bed reactor diameter
Also it increases accordingly, when setting disassembly flange is uneconomical on cylinder section and dismantles inconvenient, can be set on reactor head end socket
Inspection manhole is set, for overhauling heat removing tube beam.Baffle plate demister is set in gas vent, removes the liquid for generating and carrying secretly in gas
Drop.
200 DEG C~240 DEG C of the methyl methanol syngas temperature of slurry bed system methanol reactor, pressure 3.7MPaG~9.7MPaG out,
The conversion per pass 65~80% of CO, CO2Conversion per pass 25%~40%.
The methyl methanol syngas come out from reactor enters cyclone separator 3, further separates the drop carried secretly in gas, point
The gas phase for separating out liquid self-flowing return 2 top of paste state bed reactor come is gone, and it is pre- that the methyl methanol syngas after separation enters preheater 1
It is cooled to 120 DEG C~130 DEG C after hot mixing gas, enters back into cooler 7 and is cooled further to 30 DEG C~45 DEG C, subsequently into separation
Device 9 isolates liquid phase crude carbinol, and the crude carbinol isolated is sent to downstream methanol rectification section, and the gas phase after separation enters circulating air
Compressor 8 is forced into after 4.1MPaG~10.1MPaG be back to preheater 1 as circulating air before, mix shape with fresh feed gas
At gaseous mixture, start new circulation.
In addition, in order to avoid inert gas is accumulated inside device, it can be in separator 9 to the company of recycle gas compressor 8
Periodic off-gases discharge pipe line is set on adapter tube line, extracts one periodic off-gases out.
Since the density of catalyst is greater than the density of carrier liquid paraffin, in the certain situation of bed temperature, pressure, air speed
Under, the granularity of catalyst catalyst bed is axially distributed with certain influence, the catalyst of bulky grain bed lower part be distributed compared with
More, catalyst particle is distributed more on bed top；Air speed is divided in bed according to the granularity of raw catelyst according to catalyst
The uniform principle selection of cloth, with the progress of reaction, partial catalyst can wear broken, broken catalyst since granularity becomes
It is small, it is light-weight, it can be concentrated mainly on the top of reaction zone, the online replacement of catalyst is exactly to replace this partial catalyst.
Specific replacing options are as follows:
Open 5 top of root valve 11 and catalyst sedimentation tank of 2 reaction zone upper slurry of paste state bed reactor extraction pipeline
Gas phase return line stop valve 14, the stop valve 12 of catalyst preparation tank 6 is in close state at this time, paste state bed reactor
The slurries on 2 tops introduce catalyst sedimentation tank 5, and the gas contained in slurries returns to slurry bed system from the top of catalyst sedimentation tank 5
The gas-phase space 21 of reactor 2.
When liquid level reaches setting liquid level in settling tank 5, valve 11 and valve 14 are closed, stops extraction slurries；5~30 points of sedimentation
Clock opens valve 12, the atoleine in settling tank 5 is released from the purified liquor outlet for being located at settling tank side, wax liquor flows into catalysis
In agent preparing tank 6；Valve 12 is closed after discharge；The catalyst granules settled out is discharged from settling tank bottom nozzle.
Fresh catalyst and liquid stone is added into catalyst preparation tank 6 from the top-feed mouth of catalyst preparation tank 6
Wax prepares new catalyst pulp；After preparing, lead to inert gas into catalyst preparation tank 6 from bottom, the present embodiment uses
Low-pressure nitrogen, replaces air in catalyst preparation tank 6, and displacement gas is discharged from catalyst preparation tank top.In replacement process, inertia
Gas is used as blender gas simultaneously, and catalyst granules and atoleine are uniformly mixed.
After the completion of displacement, cutoff low nitrogen opens feed supplement valve 13, leads to elevated pressure nitrogen into catalyst preparation tank 6 from top
Gas is forced into the catalyst slurry in catalyst preparation tank 6 higher than reactor bed operating pressure by high pressure nitrogen
After 0.1MPa or more out of, reactor 2 is sent into bottom shell side；After reaching setting value, feed supplement valve 13 and high pressure nitrogen are closed, is urged
The primary online replacement of agent is completed.
Catalyst is changed to intermittently operated online, and is changed to part replacement every time, does not need device parking.
Embodiment 2
As shown in Fig. 2, when needing replacing catalyst, opening 22 top of paste state bed reactor reaction zone in the present embodiment
Slurries extract pipeline root valve 11, the gas phase return line stop valve 14 of cross-flow filter 5 and catalyst filter 10 and catalysis out
The stop valve 15 of atent solvent connecting pipeline between agent preparing tank 6.
The slurries on 22 top of reaction zone are introduced in cross-flow filter 5, primary filtration, concentrate are carried out to slurries；In slurries
The synthesis gas that the gas and new reaction contained generates returns to the gas-phase space of paste state bed reactor 2 from the top of cross-flow filter 5
21, the atent solvent filtered out enters catalyst preparation tank 6 by pressure difference；Catalyst slurry after 6 concentrate of cross-flow filter
Smart filtering is carried out into filter 10；It forms filter cake in filter 10 to draw off from bottom, the atent solvent filtered out also depends on pressure
Difference enters in catalyst preparation tank 6.
When cross-flow filter 7 and cross-flow filter 5 need to clean, slurries is kept to extract pipeline root valve 11, feed supplement valve out
13, gas phase return line stop valve 14 is in close state, and valve 15 is opened, using in high pressure nitrogen force feed catalyst preparation tank 6
Atent solvent recoils.
In addition, the present embodiment, which crosses drainage using 41 pairs of bubble points of pump, carries out forced circulation.
Remaining content is same as Example 1.
Comparative example
CN102850182A discloses a kind of slurry bed system crude carbinol synthesis system, and the catalyst in paste state bed reactor is made
Under, reaction gas, which generates, generates gas, first through cyclone separator initial gross separation atent solvent and catalyst, then through heat exchanger boiler
The cooling generation gas of water supply, byproduct steam, the atent solvent Returning reactor condensed, and on the return line of atent solvent
Setting atent solvent makes up line.
Embodiment 1 and embodiment 2 are shown in Table 1 compared with comparative example.
Table 1
As can be seen from Table 1, in slurry bed methyl alcohol synthesizing process provided by the present invention, reactor takes hot timely, bed
Temperature is stable, easy to control, and conversion per pass is high, and circulating flow rate is small, greatly reduces construction investment and plant energy consumption；Inert carrier
Entrainment is small, is not carried secretly substantially to downstream；Catalyst is replaced online, avoids the economic loss stopped by catalyst change.
Claims (8)
1. a kind of slurry bed methyl alcohol synthesizing process, it is characterised in that include the following steps:
Unstripped gas from upstream forms gaseous mixture after mixing with circulating air, heat exchange is anti-to entering after 180 DEG C~220 DEG C from bottom
The shell side for answering device (2) is contacted with the catalyst slurry in shell side and is reacted；Bubble point boiler water enters the tube side of reactor (2)；
Controlling the reaction temperature in the reactor (2) shell side is 200 DEG C~240 DEG C, and reaction pressure is 4MPaG~10MPaG, mixing
Gas air speed is 1200-H~4000-H, catalyst quality score are 0.25~0.4；
It reacts the reaction gas generated to be discharged from the top of reactor, be separated into separator；That isolates is non-gaseous from anti-
It answers and returns to the reactor in the gas-phase space (21) on device (2) top, the i.e. crude carbinol synthesis gas heat exchange of the gas phase isolated is laggard
Enter in gas-liquid separator (9), the gas phase isolated is forced into after 4.1MPaG~10.1MPaG as the circulating air, is isolated
Liquid phase be crude carbinol；
In reaction process on periodic analysis different height position catalyst slurry solid content and size distribution, reach abrasion setting
When value, catalyst slurry is extracted outward from the middle and upper part of reactor catalyst bed；Extraction amount or maximum extraction are calculated when reaching
Stop extracting catalyst slurry from inside to outside from the reactor when amount；
The slurries of extraction are filtered, atent solvent and catalyst granules are isolated；
Fresh catalyst slurry is forced into and is sent into the reaction from bottom higher than after reactor bed operating pressure 0.1MPa
In device (2) shell side；The additional amount of the fresh catalyst slurry is suitable with the catalyst slurry liquid measure extracted；
The catalyst slurry of reactor (2) the shell side extraction is introduced into settling tank (5) and is settled；The liquid phase isolated is i.e. lazy
Property solvent send in catalyst preparation tank (6), as the atent solvent of fresh catalyst, the catalyst granules discharge that settles out.
2. slurry bed methyl alcohol synthesizing process according to claim 1, it is characterised in that the unstripped gas temperature be 20 DEG C~
40 DEG C, the unstripped gas that pressure is 4MPaG~10MPaG, hydrogen-carbon ratio (H2-CO2)/(CO+CO2)=2.05~2.15；The circulation
Temperature degree is 45~70 DEG C, pressure is 4.1MPaG~10.1MPaG, mole composition (H of gaseous mixture2-CO2)/(CO+CO2)=3
~5, recycle ratio 0.7~1.1.
3. slurry bed methyl alcohol synthesizing process according to claim 2, it is characterised in that control the CO's of the reactor (2)
Conversion per pass 65~80%, CO2Conversion per pass 25%~40%.
4. slurry bed methyl alcohol synthesizing process according to any one of claims 1 to 3, it is characterised in that the bubble point boiler water
From drum (4), the steam that reactor (2) tube side generates returns to the drum (4).
5. according to claim 1 to slurry bed methyl alcohol synthesizing process described in 3 any claims, it is characterised in that from described anti-
The catalyst slurry for answering device (2) shell side to extract out, which is introduced into cross-flow filter (5), carries out preliminary separation of solid and liquid, the liquid isolated
Mutually sent in catalyst preparation tank (6) by first pipe；Catalyst slurry after concentrate, which enters, carries out essence in filter (10)
Filtering, the liquid phase isolated enter the catalyst preparation tank (6), and catalyst granules forms filter cake discharge.
6. slurry bed methyl alcohol synthesizing process according to claim 5, it is characterised in that the bubble point boiler water comes from drum
(4), the steam that reactor (2) tube side generates returns to the drum (4)；The pipe of the drum (4) and the reactor (2)
Connecting pipeline between journey entrance is equipped with pump (41).
7. slurry bed methyl alcohol synthesizing process according to claim 6, it is characterised in that the catalyst is that activation temperature is
160~250 DEG C of slurry bed system methanol synthesis catalyst.
8. slurry bed methyl alcohol synthesizing process according to claim 7, it is characterised in that the atent solvent is selected from Witon mine
Object oil or atoleine.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1272482A (en) * | 2000-04-11 | 2000-11-08 | 华东理工大学 | Three-phase bubbling slurry bed methyl alcohol synthesizing process and its equipment |
| CN104368283A (en) * | 2013-08-13 | 2015-02-25 | 中国石油化工股份有限公司 | Slurry bed reactor and applications thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1272482A (en) * | 2000-04-11 | 2000-11-08 | 华东理工大学 | Three-phase bubbling slurry bed methyl alcohol synthesizing process and its equipment |
| CN104368283A (en) * | 2013-08-13 | 2015-02-25 | 中国石油化工股份有限公司 | Slurry bed reactor and applications thereof |
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